WO2010024564A2 - Procédé de fabrication de flocons métalliques - Google Patents

Procédé de fabrication de flocons métalliques Download PDF

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Publication number
WO2010024564A2
WO2010024564A2 PCT/KR2009/004704 KR2009004704W WO2010024564A2 WO 2010024564 A2 WO2010024564 A2 WO 2010024564A2 KR 2009004704 W KR2009004704 W KR 2009004704W WO 2010024564 A2 WO2010024564 A2 WO 2010024564A2
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Prior art keywords
metal
coating
flakes
thin film
producing
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PCT/KR2009/004704
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English (en)
Korean (ko)
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WO2010024564A3 (fr
Inventor
정광춘
조현남
김동립
유지훈
Original Assignee
주식회사 잉크테크
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Application filed by 주식회사 잉크테크 filed Critical 주식회사 잉크테크
Priority to JP2011524893A priority Critical patent/JP5738763B2/ja
Priority to US13/060,857 priority patent/US8979972B2/en
Priority to CN200980133467.0A priority patent/CN102202820B/zh
Publication of WO2010024564A2 publication Critical patent/WO2010024564A2/fr
Publication of WO2010024564A3 publication Critical patent/WO2010024564A3/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/068—Flake-like particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal

Definitions

  • the present invention relates to a method for producing metal flakes, and more particularly, to a method for producing metal flakes using a coating ink containing an organometallic compound.
  • silver (Ag) is a precious metal because of its special characteristics such as excellent electrical conductivity and antibacterial ability, and has been used in various fields such as decoration, coins, tableware, home appliances, electrical and electronic products, lighting, copiers, display electrodes, electromagnetic shielding, and antibacterial properties. It is used in. In particular, despite the recent diversification and complexity of electric and electronic products, there is a demand for high quality and low price in the market.
  • metal particles such as silver, copper, nickel, and aluminum, which are mainly used in electrical and electronic products, are mostly in the form of spheres or flakes, and are used depending on the purpose.
  • the metal particles are prepared by atomization, electrochemical method, or chemical reduction, and the metal particles are mainly spherical and the spherical shape thus obtained.
  • particles in the form of metal particles in the form of flakes using a conventional ball mill US Patent Nos. 4,482,374, 4,859,241, US Patent Publication No. 2006-0207385, Japanese Patent Publication No. 2007-84860 And Japanese Laid-Open Patent No. 2007-254845 or metals are manufactured by vacuum deposition (US Patent No.
  • Such metal flake particles can be widely used for electromagnetic shielding requiring high conductivity, conductive paste for electrodes, conductive adhesive, or paints or inks requiring gloss or special colors, coloring pigments for cosmetics, and the like.
  • a method for producing metal flakes using a ball mill of spherical metal particles is the most commonly used technology, which has the advantage of being able to mass-produce relatively easily, but to produce metal flakes of uniform thickness and size,
  • the thickness and size of the metal flakes can be easily adjusted, and the metal flakes having excellent particle characteristics such as conductivity or glossiness can be manufactured, and the mass production can be performed in an environmentally friendly and economic manner.
  • the manufacturing process of the metal flakes according to the prior art has various problems such as high manufacturing cost or deterioration of various particle characteristics due to a complicated manufacturing process, while the metal flakes according to the present invention have a thickness and
  • the present invention provides a manufacturing method that can be easily controlled in size, has excellent particle characteristics such as conductivity and gloss, and can be mass-produced in an eco-friendly and economic manner.
  • the present inventors have completed the present invention by developing the thickness, light or electrical properties of the metal flakes according to the coating method, the type of substrate and the concentration of the coating metal ink composition.
  • the present invention relates to a method for producing a metal flake, and more particularly to a method for manufacturing a metal flake using a coating ink containing an organometallic compound, the present invention will be described in more detail below.
  • step b) calcining the ink coated on the substrate of step a);
  • step b) separating the metal thin film produced in step b) from the substrate;
  • step c) pulverizing the metal flakes separated in step c); Characterized in that it comprises a.
  • the present invention is characterized in that it further comprises the step of purifying the metal pulverized in step d).
  • the coating ink containing the organometallic compound of the present invention used a metal ink containing a metal complex compound having a special structure having a uniform thickness and a uniform size of the metal flakes, and has a low firing temperature described below. .
  • the preparation of the metal ink including the metal complex compound is carried out by reacting the metal ink with one or two or more mixtures selected from a metal compound and an ammonium carbamate compound, an ammonium carbonate compound or an ammonium bicarbonate compound.
  • Ammonium carbamate-based compound, ammonium carbonate-based compound or ammonium bicarbonate-based compound] a method for producing a complex has been filed in the Republic of Korea Patent Application No. 2005-34371, the same method was used in the present invention.
  • the patent application is to provide a method for producing a metal ink composition capable of forming a fine pattern of a uniform and dense thin film while having high conductivity even when fired at a low temperature, the present applicant has a simple and uniform thickness metal The method of making the flakes was devised.
  • the metal ink including the metal complex compound may include a metal complex compound obtained by reacting at least one metal or metal compound represented by Formula 1 with at least one ammonium compound represented by Formula 2, Formula 3, or Formula 4. It features.
  • M is a metal or a metal alloy, n is an integer of 1 to 10, X is absent, hydrogen, ammonium, oxygen, sulfur, halogen, cyano, cyanate, carbonate, nitrate, nitrite, sulfate, And at least one substituent selected from phosphate, thiocyanate, chlorate, perchlorate, tetrafluoroborate, acetylacetonate, merceto, amide, alkoxide, carboxylate and derivatives thereof.
  • R 1, R 2, R 3, R 4, R 5 and R 6 are each independently hydrogen; a substituted or unsubstituted C 1 -C 30 aliphatic alkyl group, alicyclic alkyl group, aryl group or aralkyl group; high molecular compound group; heterocyclic compound group; And their derivatives, and R1 and R2 or R4 and R5 may be linked to each other to form a ring.
  • the ink composition used in the present invention may be a solvent, stabilizer, dispersant, binder resin, mold releasing agent, reducing agent, or surfactant as necessary in addition to the metal complex compound and the metal or nonmetal compound or at least one of these mixtures.
  • Additives such as wetting agents, thixotropic agents or leveling agents, and the like.
  • the solvent contained in the coating solution may be selected from water, alcohols, glycols, acetates, ethers, ketones, aliphatic hydrocarbons, aromatic hydrocarbons or halogenated hydrocarbon-based solvents, specifically, water, methanol, ethanol, isopropanol, 1-meth Oxypropanol, butanol, ethylhexyl alcohol, terpineol, ethylene glycol, glycerin, ethyl acetate, butyl acetate, methoxypropyl acetate, carbitol acetate, ethyl carbitol acetate, methyl cellosolve, butyl cellosolve, diethyl Ether, tetrahydrofuran, dioxane, methyl ethyl ketone, acetone, dimethylformamide, 1-methyl-2-pyrrolidone, dimethyl sulfoxide, hexane, heptane, dode
  • the substrate used in the present invention may be any type as long as the characteristics of the present invention are met.
  • polyimide PI
  • PET polyethylene terephthalate
  • PEN polyethernaphthalate
  • PES polyethersulfone
  • nylon ylon
  • PTFE polyether ether ketone
  • Plastics such as PEEK
  • PVA polyvinyl alcohol
  • PE polyethylene
  • PP polypropylene
  • PC polycarbonate
  • PAR polyarylate
  • Rubber materials such as resins, butyl rubber, chloroprene rubber, SBR, EPR, SIS rubber, etc., glass, silica, alumina, titanium oxide, zirconia, ceria, clay, stone, talc, mica various ceramic materials such as (mica), various metals or alloy materials such as aluminum or copper, nickel, iron, zinc, stainless steel, brass, nonmetals such as carbon, graphite, carbon nanotubes, silicon, sulfur, salt, barium sulfate, or the like Metal salt compound, synthetic paper , Various papers such as photo paper, wrapping paper, corrugated paper, and various composite materials incorporating these materials can be used, and there is no need to limit in particular.
  • the shape or shape of the substrate may be powder, flake, bead, ball, fiber, film, foil, sheet, chip ( Chips, rods, wires, needles, whiskers, and the like may be used. More preferably, the metal flakes are easily attached or detached, but are not particularly limited thereto.
  • the coating method of the ink including the metal complex compound is spin coating, roll coating, spray coating, dip coating, flow coating, comma depending on the physical properties of the ink and the form of the substrate, respectively.
  • the coating thickness does not need to be particularly limited, but usually 10 nanometers to 100 microns, more preferably 50 nanometers to 10 microns is preferred. And the coating thickness can be adjusted by controlling the concentration of the ink, the coating amount or speed, etc. It is preferable to use a substrate having excellent surface roughness so as to prepare a high gloss metal flakes.
  • a mask or a patterned roll may be used for coating.
  • the gravure roll may be coated in a honeycomb structure, a mesh structure, and the like beforehand.
  • a metal ink for coating comprising a metal complex compound having a special structure of step a) on a variety of substrates, and after oxidation or reduction treatment or heat treatment, hot air, microwave, infrared, ultraviolet ray, electron beam, laser, etc. Through the process, the ink coated on the substrate may be fired.
  • the firing step may be heat treated under a normal inert atmosphere, but may be processed in air, nitrogen, carbon monoxide, or even a mixed gas of hydrogen and air or another inert gas, if necessary.
  • heat treatment of two or more steps at low and high temperatures within the above range is also good for the uniformity of the thin film. For example, it is good to process for 1 to 30 minutes at 80-150 degreeC, and to process for 1 to 30 minutes at 150-300 degreeC.
  • the thickness of the fired thin film after the post-treatment does not need to be greatly limited, but is preferably between 0.005 and 5 microns, preferably between 0.01 and 1 microns, more preferably between 0.05 and 0.5 microns. If it is less than 0.005 micron, there is a disadvantage that a uniform thin film is not formed, and above 5 micron may cause a problem that the manufacturing cost increases.
  • the steps a) and b) may be continuously performed.
  • the metal coating and firing may be repeatedly performed to repeat the process.
  • the step of preparing a thin film is also included. It is not particularly limited to be useful as a protective coating film between the metal thin film and the metal thin film when forming the multilayer thin film, but it is preferable when the detachment and drying are easy and the protective coating film characteristics are excellent.
  • the coated membrane may be easily dissolved or heated in water, alcohol, or a solvent so as to be easily separated from the substrate, which is the next step after the coating is dried.
  • Such materials include polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyolefins, urethanes, acrylics, fluorine, silicones, polyester vinyl resins and waxes.
  • step b) separating the metal thin film produced in step b) from the substrate;
  • a method of separating the metal thin film from the substrate it may be selected by a suitable method according to the substrate type and coating method of step a).
  • PI polyimide
  • PET polyethylene terephthalate
  • PEN polyethernaphthalate
  • PES polyethersulfone
  • nylon nylon
  • PTFE polytetrafluoroethylene
  • PEEK ether ketone
  • PVA polyvinyl alcohol
  • PE polyethylene
  • PP polypropylene
  • PC polycarbonate
  • PAR polyarylate
  • the metal thin film (including the multilayer thin film) produced through the sintering process of step b) is immersed in a solvent such as brine, alcohol, or acetone, methyl ethyl ketone for a predetermined time, or a method using an ultrasonic wave or a vibrator or a metal stripping machine.
  • a solvent such as brine, alcohol, or acetone, methyl ethyl ketone for a predetermined time, or a method using an ultrasonic wave or a vibrator or a metal stripping machine.
  • a solvent such as brine, alcohol, or acetone, methyl ethyl ketone for a predetermined time, or a method using an ultrasonic wave or a vibrator or a metal stripping machine.
  • the metal foil can be easily prepared by removing the metal thin film.
  • the metal thin film can be easily removed by a scraper or an air gun.
  • the deposition time of the solvent for removing the metal thin film is usually deposited for 1 minute to 5 hours, preferably 5 minutes to 3 hours, more preferably 10 minutes to 2 hours. In addition, if the deposition time is short within the above range, it may be difficult to form a metal foil of uniform thickness.
  • the metal thin film produced by ion plasma coating, electrostatic coating, electro-deposition coating, etc. is used to remove the metal thin film from the substrate by friction between particles using a ball mill.
  • the flakes can be prepared.
  • various methods such as chemical dissolution method, method of blasting gas (air, nitrogen, etc.) or liquid (water, alcohol, etc.), vacuum collection method, etc. may be used depending on the manufacturing conditions. Do.
  • step c) pulverizing the metal flakes separated in step c);
  • the method of manufacturing the metal flakes having excellent conductivity and glossiness by pulverizing the metal flakes separated in step c) to a predetermined thickness and size can be used in various ways depending on the characteristics and application fields such as particle size or shape.
  • the metal flakes produced in step c) may be prepared using a solvent such as saline, alcohol, glycol, acetone, or a fatty acid, fatty acid salt, or surfactant, to form media beads of 0.7 mm or less.
  • the fine metal flakes can be prepared by placing (media beads) in a bead mill and mixing and stirring.
  • Fine metal flakes having excellent conductivity and glossiness can be prepared by adjusting the size and thickness of the particles according to the stirring speed of the bead mill, the stirring time, the particle diameter or the material of the media beads.
  • the particle diameter of the media beads is larger than 0.7 mm, the weight of the media beads is heavy, and the pressing pressure on the particles increases, and the frequency of formation of coarse and large flake particles is dramatically increased.
  • the particle diameter of the media beads is 0.02 mm or less, the processing time in the shape of flakes is long, which may cause problems in productivity.
  • the material of the media beads it is preferable to selectively use any one of zirconia beads, alumina beads, and glass beads.
  • various methods such as a high speed mixer, a ball mill, a bead mill, an ultrasonic grinder, and a micro grinder may be used depending on the characteristics and application fields of particle size and shape. .
  • the thickness or size of the flakes produced by the above method need not be largely limited, but the thickness varies depending on the production conditions, but is preferably between 0.005 and 5 microns, preferably between 0.01 and 1 microns, more preferably between 0.05 and 0.5 microns.
  • the size of the flakes is between 0.05 and 500 microns, preferably between 0.1 and 300 microns, more preferably between 0.5 and 100 microns.
  • the glossiness of the prepared metal flakes is already determined in many cases in the firing step after coating, but also affects the grinding process. Therefore, the better the gloss, the better, and there is no need to limit in particular, and it is preferable that the reflectance of the flake is 30% or more.
  • it may further comprise the step of purifying the metal flakes pulverized in step d), which improves the purity of the metal flakes prepared in d), improves the workability and changes of the metal flakes over time or changes in the surrounding environment
  • a method for improving purity an impurity cleaning or heat treatment method using a solvent may be used.
  • Methods for controlling processability or changes over time include SiO 2 sol, fatty acids such as oleic acid, silicone compounds such as methylsilyl isocyanate, cellulose derivatives such as polysaccharide, phosphoric acid derivatives such as phosphoric acid and phosphonic acid, or the like.
  • -Merethane having 6 to 24 carbon atoms, such as hexyl, dodecyl, lauryl, hexadecyl, octadecyl, and the like. It is possible to use a method of surface treatment on metal flakes by mixing two or more kinds in various ways.
  • Surface treatment temperature of the metal flakes is usually between 50 ⁇ 500 °C, preferably heat treatment at 80 ⁇ 300 °C for the physical properties of the metal flakes.
  • the metal flakes purified by the above method can be divided into metal flakes suitable for the application field by dividing by size using a polarizing mesh which is a conventional method according to the flake size.
  • Metal flakes according to the present invention is very easy to control the thickness and size, and excellent particle characteristics such as conductivity or gloss, and can be mass-produced in an eco-friendly and economical manner.
  • the resulting copper ink had a metal content of 14.54 weight percent and a viscosity of 17 cps, metal ink solution 5.
  • metal flakes a 300mm wide and 200m long PET film with a release agent coating was prepared. Then, the metal ink 1 was coated at a speed of 20 m / s using a microgravure coating machine, and then fired at 150 to reflect 97% of the reflectivity on the PET surface. The silver coated thin film was prepared. In order to separate the prepared metal thin film, the metal thin film was peeled using an ultrasonic vibrator while immersed in 10% saline solution for 30 minutes and washed with water sufficiently to obtain silver flakes of irregular size. The metal thin film was placed in a bead mill filled with 0.1 mm zirconium media beads and stirred to prepare a metal flake having a thickness of 0.2 ⁇ m and a size of 7 ⁇ m. The uniformly prepared silver flakes were immersed in an ethanol mixed solution of 5% hexadecyl merethane (manufactured by Aldrich) for 30 seconds to prepare a finally treated silver flake.
  • a 300 mm wide and 200 m long PI film was prepared, and then the metal ink 1 was printed at a speed of 20 m / s using a microgravure coating machine to prepare a silver coated thin film having a reflectance of 97% on the PI surface.
  • the metal thin film was easily peeled off using an air gun and sufficiently washed with water to obtain silver flakes of irregular size.
  • the metal thin film was placed in a bead mill filled with 0.3 mm zirconium media beads to prepare a metal flake having a thickness of 0.2 ⁇ m and a size of 20 ⁇ m.
  • the silver flakes of uniform thickness were immersed in an ethanol mixed solution of 5% oleic acid (manufactured by Aldrich) for 30 seconds to prepare a purified silver flakes.
  • a 300mm wide and 200m length PET film with a release agent coating was prepared. Then, the metal ink 1 was coated at a speed of 20m / s using a microgravure coating machine, and then calcined at 150 ° C. to reflect a 97% reflectance on the PET surface. The silver coated thin film was prepared. Thereafter, a 20% polyvinyl alcohol resin solution was coated on the silver-coated thin film using a gravure coater and dried at a speed of 20 m / s, and then metal ink 1 was coated in the same manner as described above to prepare a double layer silver coating film.
  • the metal thin film was peeled using an ultrasonic vibrator while immersed in 10% saline solution for 30 minutes and washed with water sufficiently to obtain silver flakes of irregular size.
  • the metal thin film was placed in a bead mill filled with 0.1 mm zirconium media beads and stirred to prepare a metal flake having a thickness of 0.2 ⁇ m and a size of 7 ⁇ m.
  • the surface was first removed using ethanol, and then dried at 50 degrees for 5 minutes in a dryer. Pour the metal ink 1 (5ml) on the PET film and rotate it at 500 rpm for 20 seconds using a spin coater to form a silver coating film on the PET surface, and then bake at 150 ° C. for 5 minutes to produce a 98% silver coating thin film. It was. In order to separate the prepared silver thin film, it was immersed in 10% saline solution for 30 minutes, peeled off using an ultrasonic vibrator, and washed sufficiently with water to obtain silver flakes of irregular size. This process was repeated to prepare 10 grams of silver flakes. The silver flakes were put into a bead mill filled with 0.3 mm zirconia media beads and stirred to prepare metal flakes having a thickness of 0.3 ⁇ m and a size of 20 ⁇ m.
  • the metal thin film is peeled off using an air gun and washed sufficiently with water to obtain irregularly sized metal flakes. This procedure was repeated to prepare 10 grams of metal flakes. The metal flakes were placed in a bead mill filled with 0.3 mm zirconium media beads to prepare metal flakes having a thickness of 0.3 ⁇ m and a size of 20 ⁇ m.
  • metal ink 1 was printed at a speed of 10 m / s using a flexo coater to prepare a silver coated thin film having a reflectance of 97% on the PET surface.
  • the metal thin film was peeled using an ultrasonic vibrator while being immersed in 10% saline solution for 30 minutes and washed with water to obtain irregular silver flakes.
  • the silver flakes were placed in a bead mill filled with 0.2 mm zirconium media beads and stirred to prepare metal flakes having a thickness of 0.12 ⁇ m and a size of 10 ⁇ m.
  • the surface was first removed using ethanol, and then dried at 50 degrees for 5 minutes in a dryer.
  • the metal ink 2 was printed on the PET film using a inkjet printer equipped with a Dimatix DMP-2831 1 pl head in a dot pattern having a diameter of 15 ⁇ m, and then fired at 150 ° C. for 5 minutes to obtain a 90% reflectivity.
  • Silver coated thin film was prepared. In order to separate the prepared metal thin film, the silver flakes were peeled using an ultrasonic vibrator while immersed in 10% saline solution for 30 minutes and washed sufficiently with water, so that the thickness of the printed pattern was 0.35 ⁇ m and 15 ⁇ m in size without crushing. Got. This process was repeated to prepare 10 grams of silver flakes.
  • a glass plate for the production of metal flakes
  • the metal ink 3 was printed on the glass plate using 400 mesh screen printing, and then fired at 150 ° C. for 5 minutes to prepare a silver coated thin film having a reflectance of 45%.
  • the metal film was peeled using an ultrasonic vibrator while immersed in 10% saline solution for 1 hour, and washed sufficiently with water to obtain an irregular metal film. This process was repeated to prepare 10 grams of silver flakes.
  • the metal film was placed in a bead mill filled with 0.5 mm zirconium media beads to prepare metal flakes having a thickness of 1 ⁇ m and a size of 40 ⁇ m.
  • metal flakes a stainless steel sheet having a width of 1 meter and a width of 3 meters was prepared, and then the metal ink 1 was coated on a conveyor belt using a spray coater, and then fired at 150 ° C. for 5 minutes to obtain 95% silver. Coated thin films were prepared. In order to separate the prepared metal thin film, the metal thin film was peeled using an ultrasonic vibrator while immersed in 10% saline solution for 1 hour, and washed sufficiently with water to obtain silver flakes of irregular size.
  • metal ink 1 was placed in a fluidized bed reactor, the internal temperature was raised to 110 degrees, coated for 20 minutes while flowing, and then baked at 150 ° C. for 5 minutes to reflect 88 A silver coated thin film of% was prepared.
  • the metal thin film was peeled using an ultrasonic vibrator while immersed in 10% saline solution for 1 hour and washed sufficiently with water to obtain a metal thin film.
  • the metal thin film was placed in a bead mill filled with 0.2 mm zirconium media beads to prepare metal flakes having a thickness of 0.2 ⁇ m and a size of 10 ⁇ m.
  • a mixed solution of 3-aminopropyltriethoxysilane (manufactured by Aldrich) (30 grams) was added to the metal ink 1 (1 Kg). After the temperature was raised to 110 degrees and put into the coating while flowing for 20 minutes and then baked at 150 °C 5 minutes to prepare a metal coating thin film with a reflectance of 45%.
  • the metal thin film was peeled using an ultrasonic vibrator while immersed in 10% saline solution for 1 hour and washed sufficiently with water to obtain a metal film. The metal thin film was placed in a bead mill filled with 0.2 mm zirconium media beads to prepare a shiny pale red metal flake having a thickness of 0.2 ⁇ m and a size of 10 ⁇ m.
  • the metal ink 1 was placed in a fluidized bed reactor, the internal temperature was raised to 110 degrees, coated for 20 minutes while flowing, and then fired at 150 ° C. for 5 minutes. A 88% silver coated thin film was prepared. Thereafter, a 10% polyvinylpyrrolidone solution was coated on the silver-coated thin film using a fluid coating machine, and then metal ink 1 was coated in the same manner as described above to prepare a double-layered silver coating film. In order to separate the prepared metal thin film, the metal thin film was peeled using an ultrasonic vibrator while immersed in 10% saline solution for 1 hour and washed sufficiently with water to obtain a metal thin film. The metal thin film was placed in a bead mill filled with 0.2 mm zirconium media beads and stirred to prepare a metal flake having a thickness of 0.25 ⁇ m and a size of 10 ⁇ m.
  • metal flakes a 1m wide, 200m long polyester fiber nonwoven fabric was prepared, coated with a roll dip coating machine containing the metal ink, and then fired at 150 ° C. for 5 minutes. A silver coated thin film having a reflectance of 81% was prepared.
  • the metal thin film was peeled using an ultrasonic vibrator while immersed in 10% saline solution for 1 hour and washed sufficiently with water to obtain a metal thin film.
  • the metal thin film was placed in a bead mill filled with 0.3 mm zirconium media beads and stirred to prepare a metal flake having a thickness of 0.4 ⁇ m and a size of 20 ⁇ m.
  • Example 2 The same process as in Example 1 was carried out except that metal flakes were prepared using metal ink 4.
  • the thickness of the prepared metal flakes was 0.2 ⁇ m, the size of the metal flakes 7 ⁇ m was prepared.
  • the metal ink firing step was carried out in the same manner as in Example 16 except that the metal flakes were prepared by firing by adding a 10% hydrazine solution.
  • the thickness of the prepared metal flakes was 0.2 ⁇ m, the size of the metal flakes 6 ⁇ m was prepared.
  • Example 2 The same process as in Example 1 was carried out except that metal flakes were prepared using metal ink 5.
  • the thickness of the prepared metal flakes was 0.3 ⁇ m, the size of the metal flakes were prepared 5 ⁇ m.
  • Example 2 The same procedure as in Example 1 was carried out except that metal flakes were prepared using metal ink 6. The thickness of the prepared metal flakes was 0.25 ⁇ m, the size of the metal flakes were prepared 5 ⁇ m.

Abstract

L'invention concerne un procédé de fabrication de flocons métalliques, et plus particulièrement un tel procédé faisant appel à une encre de revêtement qui contient des composés métalliques organiques. Le procédé selon l'invention permet d'ajuster facilement l'épaisseur et la taille d'un flocon métallique, d'améliorer des propriétés comme la conductivité ou la brillance d'une poudre métallique, et d'assurer la production en série compatible avec l'environnement de flocons métalliques
PCT/KR2009/004704 2008-08-25 2009-08-24 Procédé de fabrication de flocons métalliques WO2010024564A2 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
JP2011524893A JP5738763B2 (ja) 2008-08-25 2009-08-24 金属薄片の製造方法
US13/060,857 US8979972B2 (en) 2008-08-25 2009-08-24 Method for manufacturing metal flakes
CN200980133467.0A CN102202820B (zh) 2008-08-25 2009-08-24 金属薄片的制造方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR1020080083087A KR20100024295A (ko) 2008-08-25 2008-08-25 금속박편의 제조방법
KR10-2008-0083087 2008-08-25

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WO2010024564A2 true WO2010024564A2 (fr) 2010-03-04
WO2010024564A3 WO2010024564A3 (fr) 2010-06-24

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PCT/KR2009/004704 WO2010024564A2 (fr) 2008-08-25 2009-08-24 Procédé de fabrication de flocons métalliques

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CN108864810A (zh) * 2018-07-27 2018-11-23 中山市摩尔佳包装材料有限公司 一种隐蔽磁卡用水性丝印油墨及其制备方法

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US8979972B2 (en) 2008-08-25 2015-03-17 Inktec Co., Ltd. Method for manufacturing metal flakes
CN103120042A (zh) * 2010-06-23 2013-05-22 印可得株式会社 电磁波屏蔽膜的制备方法及由其制备的电磁波屏蔽膜
CN103120042B (zh) * 2010-06-23 2016-03-23 印可得株式会社 电磁波屏蔽膜的制备方法及由其制备的电磁波屏蔽膜
US20140193656A1 (en) * 2010-11-25 2014-07-10 Samsung Electro-Mechanics Co., Ltd. Method of manufacturing fine metal powder and fine metal powder manufactured by using the same
CN102093774B (zh) * 2010-12-31 2013-11-06 清华大学 导电墨水及其制备方法
CN102093774A (zh) * 2010-12-31 2011-06-15 清华大学 导电墨水及其制备方法
US9484123B2 (en) 2011-09-16 2016-11-01 Prc-Desoto International, Inc. Conductive sealant compositions
CN103286316A (zh) * 2013-05-31 2013-09-11 尚越光电科技有限公司 一种搅拌球磨处理CuInGa粉体的方法
CN103286316B (zh) * 2013-05-31 2017-12-26 尚越光电科技有限公司 一种搅拌球磨处理CuInGa粉体的方法
CN104289721A (zh) * 2014-10-26 2015-01-21 李万青 一种聚氨酯涂料与胶黏剂的超细镍钴合金粉的制备方法
CN105922574A (zh) * 2015-11-17 2016-09-07 中研智能装备有限公司 一种等离子熔覆制造3d打印设备及方法
CN105922569A (zh) * 2015-11-17 2016-09-07 中研智能装备有限公司 一种等离子熔覆制造快速成型设备及成型方法
CN105922572A (zh) * 2015-11-17 2016-09-07 中研智能装备有限公司 一种等离子3d打印设备及方法
CN105946222A (zh) * 2015-11-17 2016-09-21 中研智能装备有限公司 一种等离子熔铸快速成型设备及成型方法
CN108864810A (zh) * 2018-07-27 2018-11-23 中山市摩尔佳包装材料有限公司 一种隐蔽磁卡用水性丝印油墨及其制备方法

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CN103862063B (zh) 2016-11-16
US20110154948A1 (en) 2011-06-30
JP5738763B2 (ja) 2015-06-24
JP2014222654A (ja) 2014-11-27
JP2012500903A (ja) 2012-01-12
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WO2010024564A3 (fr) 2010-06-24
CN102202820A (zh) 2011-09-28

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